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Cary - 100-300-4000-5000-6000i-7000 - Spectrometer - Users - Guide PDF
Cary - 100-300-4000-5000-6000i-7000 - Spectrometer - Users - Guide PDF
100/300/4000/5000/6000i
/7000 Spectrophotometers
User’s Guide
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Contents
1. Safety Practices and Hazards 5
Verifying Safe State 6
Ultraviolet radiation 6
Electrical hazards 6
Other precautions 8
Information symbols 9
Color coding 10
CE compliance 11
Electromagnetic compatibility 11
EN55011/CISPR11 11
ICES/NMB-001 12
South Korean Class A EMC declaration 12
2. Introduction 13
Installation requirements 13
Documentation 13
Conventions 14
Specifications 14
Electrical Connections 14
3. Installation 17
Starting the software 18
Software Status Bulletin 19
GPIB communications 19
Cary 100/300/4000/5000/6000i/7000 Spectrophotometers User’s
Guide 3
Contents
USB-GPIB-HS converter 19
PCI-GPIB 20
Setting up the instrument 23
Cabling 23
Power 23
Turning on the system 24
Instrument performance tests 25
Sample holders 25
Cell holders 26
Solid sample holder (Cary 4000/5000/6000i/7000 only) 29
Installing the base plate 34
Installing other accessories 34
Nitrogen purging 35
Cary 100/300 35
Cary 4000/5000/6000i/7000 35
Removing the sample compartment base 38
Cary 100/300 38
Cary 4000/5000/6000i/7000 38
4. Maintenance 39
Cleaning 40
Source lamps 40
Fuses 41
Spare Parts 42
Ultraviolet radiation
The deuterium (standard in all instruments) and mercury lamps (if
fitted) in the instrument emit hazardous ultraviolet (UV) radiation.
This radiation can cause serious damage to eyes. NEVER look
directly at either lamp and NEVER operate either lamp unless it is
correctly mounted in the lamp turret (Cary 4000/5000/6000i/7000
only) and the turret is correctly mounted in the instrument.
Electrical hazards
The Cary 100/300/4000/5000/6000i/7000 instruments and some
accessories contain electrical circuits, devices, and components
operating at dangerous voltages. Contact with these circuits, devices
and components can cause death, serious injury, or painful electrical
shock.
Other precautions
Both the deuterium and the visible lamps operate at high
temperatures, and touching either of these lamps may result in
burns. Before replacing a lamp that has been lit, switch off the
spectrophotometer and either ensure that the lamp has cooled, or
protect your fingers from burns.
Do not block the ventilation grilles on the spectrophotometer and
accessories. Consult the manuals supplied with your computer,
monitor and printer for their specific ventilation requirements.
Use of the Cary system and accessories may involve materials,
solvents and solutions which are flammable, corrosive, toxic or
otherwise hazardous.
Careless, improper, or unskilled use of such materials, solvents and
solutions can create explosion hazards, fire hazards, toxicity and
other hazards which can result in death, serious personal injury, and
damage to equipment and property.
ALWAYS ensure that laboratory safety practices governing the use,
handling and disposal of such materials are strictly observed. These
safety practices should include the wearing of appropriate safety
clothing and safety glasses.
Information symbols
The following triangular symbols appear in conjunction with
warnings on the spectrometer and associated documentation. The
hazard they depict is shown below each symbol:
I Mains power on
Fuse
Focus
Vertical adjustment
Horizontal adjustment
Color coding
The various indicator lights appearing on Agilent instruments and
associated accessories are color-coded to represent the status of the
instrument or accessory.
A green light indicates the instrument is in normal/standby
condition.
An orange light indicates that a potential hazard is present.
A blue light indicates that operator intervention is required.
A red light warns of danger or an emergency.
CE compliance
Agilent Cary instruments have been designed to comply with the
requirements of the Electromagnetic Compatibility (EMC) Directive
and the Low Voltage (electrical safety) Directive (commonly referred
to as the LVD) of the European Union. Agilent has confirmed that
each product complies with the relevant directives by testing a
prototype against the prescribed EN (European Norm), IEC or CISPR
standards.
Proof that a product complies with the directives is indicated by:
The CE marking appearing on the rear of the product.
The documentation package that accompanies the product,
containing a copy of the Declaration of Conformity. This
declaration is the legal declaration by Agilent that the product
complies with the directives and also shows the EN standards to
which the product was tested to demonstrate compliance.
Electromagnetic compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all ISM equipment in
which there is intentionally generated and/or used conductively
coupled radio- frequency energy which is necessary for the internal
functioning of the equipment itself.
Class A equipment is equipment suitable for use in all
establishments other than domestic and those directly connected to a
low voltage power supply network which supplies buildings used for
domestic purposes.
This device complies with the requirements of CISPR11, Group 1,
Class A as radiation professional equipment. Therefore, there may be
potential difficulties in ensuring electromagnetic compatibility in
other environments, due to conducted as well as radiated
disturbances.
Operation is subject to the following two conditions:
1 This device may not cause harmful interference.
ICES/NMB-001
This ISM device complies with Canadian ICES- 001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
2. Introduction
Installation requirements ......................................... 13
Documentation ........................................................... 13
Specifications14
Electrical Connections .............................................. 14
Installation requirements
Before receiving your Agilent Cary instrument, you will have been
provided with a Cary Site Preparation Guide, which describes the
environmental and operating requirements of the Cary system. You
must prepare your laboratory according to these instructions before
the Cary can be installed. You should keep the site preparation guide
for future reference. If you misplace your copy, you can obtain a
replacement from your local Agilent office.
Documentation
You have been provided with the following documentation to help
you set up and operate your Cary 100/300/4000/5000/6000i/7000
system:
This user’s guide, with safety practices and hazards information,
instructions for installing and maintaining the components of the
Cary hardware and software, and troubleshooting information
Extensive Help (provided with the Cary WinUV software)
containing context-sensitive Help, step-by-step instructions for
frequently performed analyses, and operating instructions.
Conventions
The following conventions have been used in procedures throughout
the documentation:
Menus, menu items, buttons and check boxes have been typed in
bold. For example, ‘click OK’ and ‘From the Edit menu, choose
Copy’.
ALL CAPITALS indicate keyboard commands. For example,
‘press ENTER’ and ‘press SHIFT+F8’.
A Note is used to give advice or information.
A Tip is used to give practical hints to help you achieve the best
possible performance from your instrument.
Specifications
See the Cary 100/300/4000/5000/6000i Site Prep Guide for all
specifications.
Electrical Connections
Rear
IEEE 488 (GPIB Cary 100/300/4000/5000/6000i/7000 system
connection)
Sample compartment
15-pin D-range connector with 2 high voltage pins: -1000 VDC,
+125 VDC (Cary 4000/5000/7000), +85 VDC (Cary 6000i), -1150 VDC,
125 VDC (Cary 100/300)
When the Accessory Controller Board is fitted in the Cary 100/300
and for all Cary 4000/5000/6000i/7000 instruments:
Three connectors for accessories in the sample compartment
(low voltage DC, and digital lines)
One connector for accessories on the front of the instrument
(identical to one of the connectors described above).
NOTE For more information, refer to the Accessory Controller Board operation manual,
in the Help.
3. Installation
Starting the software ................................................ 18
Software Status Bulletin .......................................... 19
GPIB communications............................................... 19
Setting up the instrument ........................................ 23
Turning on the system .............................................. 24
Instrument performance tests ................................. 25
Sample holders ........................................................... 25
Installing the base plate ........................................... 34
Installing other accessories ..................................... 34
Nitrogen purging ........................................................ 35
Removing the sample compartment base ............. 38
NOTE Ensure the software registration is completed by the user of the Agilent Cary UV-
Vis-NIR spectrophotometer. For further information, refer to the Software
Registration Help.
NOTE The Product Key is found on the cover of the Agilent Cary WinUV software CD
case.
5 Complete all the fields on the ‘Product Details’ page. Click Next.
6 Complete all the fields on the ‘Work Environment Details’ page.
Click Register.
7 A dialog appears stating ‘Your Agilent Software Registration has
been successful’.
NOTE If your computer is not connected to the internet, refer to the Software
Registration Help for further information.
8 The application will now open, and you can collect your data.
TIP To familiarize yourself with the Cary WinUV software, browse the Help after
installing the software.
GPIB communications
Either a GPIB communications card or a USB-GPIB-HS converter must
be installed in your computer to interface the computer and Cary
spectrophotometer. See Page 19 for information on installing the PCI-
GPIB communications card or for connecting the USB-GPIB-HS
converter.
CAUTION The components on the communications card and computer are highly static-
sensitive. To avoid damaging these components, you must drain any static
charges from your body before installing the board, and prevent the generation of
any new static charges during the installation. This can be done by wearing an
ESD (electrostatic discharge) wrist strap attached to a grounding point. You can
obtain a disposable ESD strap from Agilent; otherwise you can obtain one from
your local electronics supplier.
USB-GPIB-HS converter
To install a National Instruments USB-GPIB-HS converter:
NOTE Ensure that the Cary WinUV software has been installed. Refer to Page 17.
PCI-GPIB
To install a National Instruments PCI-GPIB communications card:
NOTE Ensure that the Cary WinUV software has been installed. Refer to Page 17.
3 Attach one end of the ESD strap to a bare metal part of the
computer chassis and wrap the other end around your wrist.
6 Press the card firmly into the empty computer slot. The gold edge
connectors should slide firmly into the matching sockets of the
computer slot. Secure the card with the screw.
8 Connect the cable between the instrument and the computer (one
end plugs into the interface board in the computer, and the other
plugs into the socket in the rear of the instrument).
9 Connect the computer to the mains power
10 Turn on the computer.
Locate the PC keyboard and mouse for ergonomically correct access.
Cabling
The printer (4) and spectrophotometer (1) are connected to the
computer via cables that plug into the back of the computer. Consult
your monitor and printer manuals for details of their cabling
requirements.
The spectrophotometer is connected to the computer by a shielded
IEEE-488 cable (3). One end of this plugs into the interfacing board
(2) in the computer and the other plugs into the socket at the rear of
the spectrometer.
Power
Requirements
Power requirements are detailed in your Cary Site Preparation
Guide, and in the ‘Specifications’ section on Page 14. Thoroughly
read this information before connecting the Cary system to the power
supply.
Consult the manuals supplied with your printer and computer for
their power requirements.
Connection
The mains power connection is located at the rear of the instrument.
Before connecting the instrument to the power supply, ensure both
the instrument and the power supply are turned OFF, and that the
voltage selector switches on the instrument rear panel (Cary 100/300
only) are set to the correct mains power supply voltage (refer to the
table on the rear panel of the instrument).
You should also check the fuses before connecting the instrument to
the mains power supply to make sure they are the correct type and
rating for your location. There are two operator accessible fuses
located at the rear of the instrument. See Page 41 for instructions on
how to check the fuses.
To connect the instrument to the mains power supply, plug the mains
power cord into the back of the instrument and the free end of the
power cord into the mains power supply, and then switch on the
mains power supply.
CAUTION If you have a Cary 300 instrument, you MUST loosen the transit screw in the
wavelength drive before turning on the instrument. Turning on the instrument
without releasing this screw will damage the instrument. Use a flat-head
screwdriver to loosen the transit screw approximately three turns. (The transit
screw is located at the rear of the instrument, on the right side when viewed
from the rear, and is clearly labeled).
NOTE For optimum performance, allow your Cary instrument to warm up for 2 hours
before use.
Sample holders
This section describes how to install the sample holders in your
instrument. Unless otherwise stated, removal procedures are the
reverse.
Before the solid sample or single sample holders can be installed into
the Cary 4000/5000/6000i/7000 instrument, they must be mounted
onto the base plate. The base plate is then installed into the
instrument using the LockDown mechanism (see Page 34).
Cell holders
Cary 100/300
The Cary 100/300 comes with a cell holder base and two single cell
holders. These are shipped installed in the sample compartment;
however, if removed, they can be reinstalled.
To reinstall the cell holder base and cell holders:
1 Open the sample compartment lid and remove the front panel.
2 Loosen the two black screws at the back of the sample
compartment and remove the black screw on the front right side.
Note the position of the locating pin at the front left side of the
sample compartment.
3 Hold the cell holder base so that the black, solid section is away
from you. Note the key holes at the back of the cell holder base.
4 Carefully place the cell holder base in the sample compartment
and slot the keyholes under the two raised black screws at the
back of the compartment. The front of the cell holder base should
fit over the locating pin.
5 Tighten the raised black screws and also secure the black screw
at the front right side of the compartment.
6 Holding a cell holder so that the notched section is to the right
(see Figure 2), carefully place the cell holder over the two
locating pins on the cell holder base in the reference beam.
Figure 2. Top view of cell holder with notched section to the right
7 Tighten the thumbscrew.
8 Repeat Steps 6 to 7 for the sample beam.
The cell holders are now installed and ready for use.
Cary 4000/5000/6000i/7000
The Cary 4000/5000/6000i/7000 comes with two single cell holders.
All instruments come with base plates as standard.
NOTE The single cell holders must be installed onto the base plate before they can be
installed into the sample compartment of the instrument. For instructions on
installing the base plate into the sample compartment, see Page 34.
NOTE If you are operating in normal or double mode, the sample position is at the
front of the sample compartment. If you are operating in reverse mode, the
sample position is at the rear.
4 Place a cell holder on the cell holder base (it will only fit one
way) and tighten the thumbscrew.
5 You can now install the base plate into the sample compartment
of the instrument (see Page 34).
6 Once the base plate is installed, the cell holder must be aligned in
the light beam (see the next section).
Figure 4. Single cell holder aperture. The thatched area in the middle shows the
beam image
1a
Figure 5. Solid sample slide showing V-holder (1) and spacer (1a)
Alternatively, you can attach a locking plate to a solid sample slide
using the two 40 millimeter pins, as shown in Figure 6. This
arrangement is suitable for large samples.
2b
2a
Figure 6. Solid sample slide (2) with pins (2a) and locking plate (2b)
The solid sample holder must be fitted to the LockDown base plate
before being installed in the instrument.
To install the solid sample holder onto the base plate:
1 Screw the optical rails into the removable base plate using the
1/8 inch hexagonal balldriver to tighten the two locating screws.
The notch should be on the right side. (Two post clips on the
underside of the plate identify the back of the base plate.)
TIP You may find it more convenient to have a set of optical rails and solid sample
holders permanently installed onto a base plate. You can then simply install and
remove the base plate as required.
3a
3b
3c
Figure 7. Optical rails showing the locating screw (3a), notch (3b) and
adjustment screw (3c)
2 Place the other set of rails in the reference position with the
notch towards the left side of the base plate. The setup procedure
for both sample and reference solid sample holders is otherwise
the same.
NOTE If you are operating in normal or double mode, the reference position is at the
rear of the sample compartment. If you are operating in reverse mode, the
reference position is at the front.
3 Loosely clamp the slide holder to its base. Insert the slide holder
onto the optical rails but do not tighten the clamping screw.
4a
4b
Figure 8. Slide holder showing the side screw (4a) and clamping screw (4b)
4 Insert the solid sample slide with attached V holder or locking
plate into the center of the slide holder and tighten the side
screw.
TIP Place the solid sample slide into the slide holder so that the slide masks the
light beam before it reaches the sample. This minimizes scattering of the light
beam.
5 You must now install the base plate into the sample compartment
(see Page 34) and then align the accessory (see the next section).
NOTE You can use a polarizer/depolarizer with the solid sample holder. These are
available from Agilent.
Extra slide holders are also available. Two of these can be screwed
into the ends of the optical rails.
If you want to use liquid rather than solid samples with your Cary
instrument, you will first need to purchase a cell holder base and a
single cell holder from Agilent.
Alternatively, you can buy a variable pathlength cell holder (see
Figure 9) available from Agilent. This will slot into your solid sample
holder base.
Figure 9. Optional accessories for the solid sample holder. Variable pathlength
cell holder (left) and side mounted slide (right)
Position the sample so that the center of the sample sits in the center
of the sample compartment (see Figure 10). The sample should be
horizontally and vertically centered.
Figure 10. Aligning the sample in the sample compartment. Left: Sample
compartment from above. The dotted line indicates the middle of the
compartment. Right: Middle of the sample compartment when viewed from the
side
Nitrogen purging
Cary 100/300
The sample compartment of the Cary 100/300 can be nitrogen purged
if the Extended Sample Compartment is fitted. The nitrogen supply
should be attached to the inlet tubes beneath the Extended Sample
Compartment.
Refer to the Extended Sample Compartment operating instructions
in the Help for further information.
Cary 4000/5000/6000i/7000
The nitrogen purging system is NOT supplied by Agilent, but the
following items are available from appropriate commercial suppliers:
Nitrogen
Ultra-high purity liquid nitrogen, for example Nitrogen 5.0, (in
conjunction with a heat exchanger) is recommended because it is less
expensive than compressed nitrogen and is usually of better quality.
If compressed nitrogen must be used, the gas must be dry, oil-free
and uncontaminated.
CAUTION Never use compressed nitrogen from a supplier who uses oil or water in the
compression process. Such processes invariably leave fine particles of oil
suspended in the nitrogen, which will form an oily deposit on optical surfaces.
Use nitrogen from a supplier who fills containers from immersion pumps
lubricated with liquid nitrogen.
NOTE The instrument warranty will be void if damage is caused by the use of
unsatisfactory nitrogen.
Supply tubing
Use clean, flexible plastic (polyvinyl chloride (PVC) or equivalent)
tubing of 6 millimeter (1/4 inch) internal diameter. Never use rubber
tubing because it may be treated internally with talc that can be
blown into the optical system.
CAUTION Never use rubber tubing, because it may be treated internally with talc that can
be blown into the optical system.
Procedure
You may need to purge the instrument with nitrogen under the
following circumstances:
NOTE If samples are frequently changed, you may need to increase the flow rate
through the sample compartment.
NOTE You can gauge the success of purging by scanning for oxygen in the UV-Vis
region and by scanning for water vapor in the NIR region (Cary 5000/6000i
/7000 only).
Cary 100/300
The Cary 100/300 has a rectangular base plate in the sample
compartment to protect the connectors from spills. You will need to
remove this plate when you install an accessory that plugs into one of
the sockets underneath the sample compartment.
The plate should be replaced in the sample compartment when the
accessory is removed to prevent damage to the connectors from
liquid spillage.
Cary 4000/5000/6000i/7000
The base of the Cary 4000/5000/6000i/7000 sample compartment is
completely removable. This allows for large apparatus to be
positioned in the sample compartment.
NOTE Once the floor of the sample compartment has been removed, the optical
alignment with respect to the floor has been lost. Before performing any
microcell analyses, you will need to realign the optics.
4. Maintenance
Cleaning ....................................................................... 40
Source lamps .............................................................. 40
Fuses ............................................................................ 41
Spare Parts .................................................................. 42
NOTE This section refers only to maintenance procedures for the Cary
spectrophotometer. You should refer to your computer and printer manuals for
their maintenance procedures.
Cleaning
Any spills in the sample compartment should be immediately wiped
up and any deposits on the sample compartment windows should
also be removed.
The exterior surfaces of the Cary spectrophotometer should be kept
clean. All cleaning should be done with a soft cloth. If necessary, this
cloth can be dampened with water or a mild detergent. Do not use
organic solvents or abrasive cleaning agents.
Source lamps
Instructions for how to change and align both the visible and
ultraviolet (UV) lamps for Cary instruments are included in the Help
provided with the software.
For both lamps the following safety precautions should be observed:
CAUTION Care must also be taken when removing lamps. Touching the glass envelope of
either the deuterium or visible lamp will reduce its efficiency. NEVER touch the
glass surfaces of new lamps. ALWAYS handle a lamp by its base, using a soft
cloth.
Fuses
The spectrophotometer contains two fuses, which are located at the
back of the instrument. To replace a fuse, disconnect the
spectrophotometer from the power supply, and replace the blown
fuse with one of the type and rating as indicated in the Site
Preparation Guide or on the rear of the instrument.
NOTE For safety reasons, any other internal fuse or circuit breaker is not operator-
accessible, and should be replaced only by Agilent authorized personnel.
To check a fuse:
1 Disconnect the instrument from the mains power supply.
2 Undo the fuse cap by pressing the cap and turning it counter-
clockwise.
3 Carefully pull out the cap. The fuse should be held in the fuse
cap.
4 Check that the fuse is the correct type and is not damaged. If
necessary, replace the fuse.
5 Place the fuse into the cap, push the cap in, and then turn the cap
clockwise.
6 Reconnect the instrument to the mains power supply.
NOTE If a fuse repeatedly blows, it may indicate other problems with the Cary
instrument. A service call may be required.
Spare Parts
For information about spare parts and their part numbers, refer to
the Agilent website: www.agilent.com
In This Book